Distillation



Feb. 16, 1937. E. G. RAGATZ 2,070,864

' DISTILLATION Filed Oct. 19, 1953 YAPORS FIXED GAS CONDENLS'A TE [PE 65/ W/VG TANK OIL FREE- LSOLYEA/T' ZPEFL UX PRESSURE STILL YAPOPS' FEED 01L g? SOLVENT Y4 C U UM AS TILL 4f WICUUM PUMP g, COMPRESSOR C ONDE NBSA TE HEATER VAPOR HEA TEE SEPARA TOR sou/EN T 1x 'LN'IOK FREE-01L j Edward 6'. Raga Z Patented Feb. 16, 1937 UNITED STATES PATENT OFFICE to Union Oil Company of California,

Los

Angeles, Calif., a corporation of California Application October 19, 1933, Serial No. 694,300

\ 3 Claims.

This invention relates to fractional distillation. The invention relates more particularly to the recovery of a solvent from solution in a hydrocarbon oil, by fractional distillation.

In many solvent extraction processes the relative boiling ranges ofthe oil and solvent are such that, at allowable distillation temperatures, a complete separation of the solvent and oil cannot be accomplished in a single still which is operated at the same time under suflicient pressure to condense the vaporized solvent at available cooling water temperatures. Consequently, under these conditions it is necessary to employ a twostage process of distillation in which the first is a pressure distillation stage of limited temperature range, and the second a stage of distillation which is conducted at a pressure materially lower than the first.

If the relative boiling ranges of solvent and oil are such that no appreciable quantity of oil is vaporized in the low pressure distillation stage,

the solvent vapors therefrom can be compressed and condensed in the solvent condenser of the pressure stage. However, in many cases the relativeboiling ranges of solvent-and oil are such that large amounts of oil are vaporized along with solvent in a low pressure stage and this results in a solvent condensate which is contaminated with appreciable quantities of oil even though the vapors leaving this stage are cooled previous to condensation. This condition can be overcome by introducing the vapors from the low pressure distillation stage into an intermediate point in the pressure distillation column.

Objects of this invention are therefore to provide a process and apparatus whereby complete separation of solvents and oils, having relatively close boiling ranges, can be accomplished; wherein neither the separated solvent nor oil will be contaminated with the other; wherein condensation of recovered solvent can be accomplished at available cooling temperatures, and wherein at the same time the highest temperatures employed in the distillation are well below those at which undesirable chemical actions begin to take place. These objects are attained in general, according ,to the invention by providing a two-stage distilla-' of the solvent from the said oil, and the return of the solvent vapors along with oil vapors from the said low pressure distillation stage to an intermediate point in the first pressure distillation stage and the withdrawal of the solvent-free oil from said low pressure distillation stage, and 5 the withdrawal of oil-free solvent from'the pressure condenser.

The invention broadly stated comprises a process and apparatus, for the recovery of solventfree oil and oil-free solvent by distillation wheren the solvent-oil solution is subjected to a twostage distillation process.

The invention more specifically resides in a process and apparatus 1? rthe recovery of solvent and oil from a solventil'solution, by two-stage distillation wherein the stages are operated at different pressures, and wherein the first stage is operated at a limited temperature and the same time at a pressure suflicient to allow condensation of the vaporized solvent at available cooling water temperatures and the second stage is operated at a pressure low enough to allow vaporization of all of the solvent remaining in the oil, and wherein the resultant vapors from the low pressure stage, which may contain vaporized oil, are introduced into the high pressure stage for further fractionation, separation, and final condensation under pressure in the pressure condenser, and wherein solvent-free oil is withdrawn from the low pressure stage still and oil-free solvent withdrawn from the high pressure condenser. v i

Other objects, advantages and features of the invention willbe evident hereinafter.

The accompanying drawing illustrates one embodiment of the invention in which I0 is a pressure fractionating column in communication with a pressure still ll and having an intermediate feed inlet connection l2, top vapor' outlet connection I3, reflux return inlet connection l4, still heating element or coil l5, still bottoms outlet connection l6, intermediate vapor inlet connection 11, and intermediate condensate inlet l8. The top vapor outlet connection l3 leads to a pressure condenser 29, and line 2| conducts pres- I sure condensate from the condenser to a condensate receiver 22. The reflux inlet I4 is connected to the condensate receiver through pipes 24 and 26. Pump 25 serves to withdraw condensate from receiver through line 24 and to force it through line 26 to the said reflux inlet Ill to the pressure still. ,A low. pressure fractionating column 30 in com-, municatin with 'low pressure still 3| receives its feed through line I6, pressure reducing valve 5 3| and top feed inlet connection 32. A top vapor outlet 34 leads to a cooler 35 which is in turn connected through a vapor and condensate line 36 to a condensate and vapor-receiving and separating tank 31. The vapor space of tank 31 is connected to the pressure still vapor inlet connection l1, through vapor line 42, and compressor 4|. The bottom liquid'space of tank 31 isconnected to'the pressure still condensate inlet con- Q the pressure fractionating nection i8, through line 33 and pump 38.

Bottoms from thelow pressure still .3l are withdrawn through the outlet connection 40. Pressure condensate is withdrawn from the condensate receiver 22 through line 23.

The operation is as follows:

A solution of oil and solvent is introduced into column In through the feed inlet connection I 2 and passed down through the lower portion of the column in countercurrent contact with upward. rising heated vapors from the heated bottoms in still ll. Heat is supplied to the still I i through suitable heating means such as heating coils i 5 through which a fluid at high temperature may be circulated. The vapors stripped from the oil-solvent feed in the lower portion of the column together with the vapors from the still continue upward through column in, are fractionated therein in counterent contact with downward flowing reflux condensate and finally the fractionated solvent .vapor is withdrawn through vapor outlet connection i3 and cooled and condensed in pressure condenser 20. The pressure condensate passes from the condenser 20 through line 2| into condensate receiver 22 densate and flxed gases takes place and from where, through line 23, the oil-free solvent condensate is withdrawn. A portion 01' the solvent condensate from tank 22 is Feturn umn for reflux by means ofpump through lines 24 and 23 and inlet.

Fixed gases may e still bottoms from which a major portion of the solvent has been vaporized but which still retains remnants of solvent, owing to the impossibility of vaporizing all of it at the operating temperature and pressure therein, is withdrawnfrom still H through bottoms outlet l6 and flows, due to the tween the stills, through pressure reducing valve 3| and line 32 into the top of the low pressure fractionating column 30. The oil containing solvent is stripped, at reduced pressure in column 30, of the remaining remnants of. solvent'by countereurrent contact with rising heated oil vapors from still 3|. Heat is supplied to still 3i by suitable heating means such as a heating coil 33 through which, a suitable heating fluid may be circulated. a

At the reduced pressure of operation in the column and still 3| all of the solvent is vaporized and stripped from the oil in thestill bottoms, but under this condition of operation with many solutions of solvent and oil, a portion of the oil is also vaporized and is carried overhead with the solvent vapors to the condenses. Thus, the solvent vapors containing oilvapors are withdrawn through vapor line 34 and cooled and partially condensed in cooler 35 in indir t heat exchange with a suitable cooling medium. The condensate and vapors pass from the through line 36 into the condensate and vapor separator 37. The condensate and vapors received in the separator 37 each contain both oil and solvent and these may be returned to the where separation of con-.-

ed to the sure of operation in the pressure this condition at the still .from still 3| through line pressure stage for refractionation. The condensate is withdrawn from the bottom of separator 31 and returned by means of pump 38 tlfiough line 39 and inlet connection l8 into an intermediate portion of the pressure fractionating cdlumn ill. The vapors are'removed from the top of the separator 31 and compressed by compressor 42 and returned through'line 42 and inlet to an intermediate portion of the said pres sure fractionating column.

.The condensate and vapors from separator 31 may be returned together through a single return line by employing apump capable of handling both liquids and vapors at the same time, or when employing such a pump the condensate and vapors may be returned directly from the cooler 35 to the pressure fractionating column l0.

The condensate and vapors containing oil and solvent are thus returned to the pressure fractionating stage II] where they are refractionated and the solventyapors finally separated and condensed in the pressure condenser 20. k Solvent-free oil is withdrawn from the bottom of the vacuum still 3| through line 40.

The fractionating columns illustrated at l 0 and 30 are of the conventional type employing perforated or bubble fractionating trays.

A typical example of operation according to the invention may be outlined as follows:

A solution of gasoline and sulphur dioxide as obtained in the Edeleanu solvent process of treating, is introduced either cold or with some preheating, into the pressure fractionating column. The gasoline may be ordinary motor fuel and'ha've an initial boiling point of 400 F. at '71 lbs. per square inch absolute and the pure sulphur dioxide will have a vapor pressure of 71 lbs. per square inch absolute at 90 F. The pres fractionating column and still may then be maintained at 71 lbs per square inch absolute and condensation of practically pure sulphur dioxide accomplished in the pressure condenser 20 with a cooling water temperature slightly below 90 F. The solvent-oil solution and reflux condensate entering the still ll could be stripped .of all the solvent and a solvent-free oil obtained therefrom by maintaining a" temperature there of 400 F. But this is undesirable for a number of reasons, chief vamong them being the tendency of the constituents tmdergoing distillation at that temperature, to undergo undesirable chemical reaction with .one another, and also the usual inconvenience of obtaining heating fluid at this high temperature. "Steam at about 225 F. may be conveniently and safely used to heat the said still I i and under pressure of 71 lbs. per square inch absolute a bottoms of 051 containing approximately four percent by volume, of liquid sulphur dioxide will be withdrawn therefrom.

The bottoms containing four percent liquid sulphur dioxide may then be introduced into the low pressure column 30 through line i6, valve 3| and inlet 32, and there stripped of the remaining liquid sulphur dioxide at a pressure of 6 inches vacuum at a still temperature of 225 inches vacuum and 225 F. the oil withdrawn will be practically solvent free.

The overhead vapors for the low pressure still withdrawn through line 34 will under these conturned, subsequent to recompression, to the pressure column for further fractionation as described hereinbefore.

The foregoing is merely illustrative of one apparatus and process and the invention is not to be limited thereby but may include any process and apparatus which accomplishes the same within the scope of the invention.

I claim:

- 1. A process for making a sharp separation between high and low vapor pressure components of a feed mixture where their completezseparation cannot be accomplished at a single pressure due to heater and condenser temperature limitations, comprising iractionally distilling the feed mixture in a high pressure stage under pressure sufiicient to allow condensation of the substantially pure high vapor pressure overhead component at normal cooling water temperatures and producing a low vapor pressure bottoms component containing a sufllcient quantity of the residual high vapor pressure component in solution to develop the required condenser pressure, fractionally distilling sai'd bottoms in a low pressure stage under pressure sufficiently reduced to strip the residual high vapor pressure component A from the oil and to produce a low pressure stage component bottoms substantially free from the high vapor pressure component and an overhead stripping vapor mixture of the two components, condensing that portion of the said overhead stripping v'apors which is condensible at normal cooling water temperatures, returning the resultant partial condensate to an intermediate .sta e in the high pressure fractionation stage, compressing and returning the uncondensed portion of the.

said low pressure overhead vapors to an intermediate stage in the high pressure fractionator and withdrawing from the high pressure fractionation 2. A process for making a sharp separation between high and low vapor pressure components of a feed mixture comprising fractionally distilling the feed mixture in ahigh pressure fractionating column under pressure suillcient to allow condensation of the substantially pure high vapor pressure overhead component at normal cooling water temperatures and producing a low -vapor pressure bottoms component containing a suflicient quantity of the, residual. high vapor pressure component in solution to' develop the required condenser pressure, fractionally distilling said bottoms in a low pressure stage under pressure sufllciently reduced to strip the residual high vapor pressure component from the oil and to produce a low pressure stage component bottoms substantially free from the high vapor pressure component and an overhead stripping vapor mixture of the two components, condensing that returning the uncondensed portion of the said low' pressure overhead vapors to an intermediate stage in the high pressure fractionating column and withdrawing from the high pressure frac tionating column an overhead high vapor pressure condensate substantially free from the low vapor pressure component and withdrawing a bottoms from the low pressure fractionation stage substantially free from the high pressure component.

3. A process for making a sharp separation of a high vapor pressure solvent and a low vapor pressure hydrocarbon oil from a feed mixture thereof comprising fractionally distilling the feed mixture in a high pressure fractionating column under pressure suflicient to allow condensation of the substantially pure high vapor pressure solvent overhead vapors at normal cooling water temperatures and producing a low vapor pressure hydrocarbon oil bottoms component containing a sufiicient quantity of the residual high vapor pressure solvent in solution to develop the required condenser pressure, fractionally distilling said bottoms in a low pressure stage under pressure sufflciently reduced-to strip the residual high vaporpressure solvent from the oil and to produce a low pressure stage hydrocarbon oil bottoms substantially free from the high vapor pressure solvent and an overhead stripping vapor mixture of hydrocarbon oil and solvent, condensing that portion of the said overhead stripping vapors which is condensible at normal cooling water temperatures, returning the resultant partial condensate to an intermediate stage in the high pressure fractionating column, compressing and returning the uncondensed portion of the said low pressure overhead vapors to an intermediate stage in the high pressure fractionating column "and withdrawing from the high pressure fractionating column an overhead high vapor pressure solvent condensate substantially free from the low vapor pressure hydrocarbon oil and with;

EDW. G. RAGATZ. 

